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1、Reference number ISO 14899:2001(E) ISO 2001 INTERNATIONAL STANDARD ISO 14899 First edition 2001-02-15 Plastics Polyols for use in the production of polyurethane Determination of basicity Plastiques Polyols pour la production du polyurthanne Dtermination de la basicit Copyright International Organiza
2、tion for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 08:41:01 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 14899:2001(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance wit
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6、n may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 ? CH-1211 Geneva 2
7、0 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.ch Web www.iso.ch Printed in Switzerland ii ISO 2001 All rights reserved Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 08:41:0
8、1 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 14899:2001(E) ISO 2001 All rights reservediii ContentsPage Foreword.iv Introduction.v 1Scope 1 2Normative references1 3Terms and definitions .1 4Principle2 5Sampling.2 6Interferences 2 7Reagents.2 8Apparatus.2 9Procedure
9、.3 10Expression of results 3 11Precision and bias.4 12Test report4 Bibliography5 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 08:41:01 MDTNo reproduction or networking permitted without licens
10、e from IHS -,-,- ISO 14899:2001(E) iv ISO 2001 All rights reserved Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical
11、 committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with
12、 the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the m
13、ember bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsi
14、ble for identifying any or all such patent rights. International Standard ISO 14899 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ
15、/9980755100 Not for Resale, 04/23/2007 08:41:01 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 14899:2001(E) ISO 2001 All rights reservedv Introduction This method is for the determination of trace amounts of basicity in polyether polyols, which are used in the prepara
16、tion of polyurethane prepolymers and polyurethane products. Knowledge of this value is important to prevent gelation during prepolymer production and to control reaction rates during polyurethane preparation. The method, known as the CPR (controlled polymerization rate) analysis, has become an accep
17、ted industry practice, a version of which has been published as part of JIS K 1557. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 08:41:01 MDTNo reproduction or networking permitted without lic
18、ense from IHS -,-,- Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 08:41:01 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARDISO 14899:2001(E) ISO
19、2001 All rights reserved1 Plastics Polyols for use in the production of polyurethane Determination of basicity WARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purport to address all of the safety problems, if any, associate
20、d with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. 1Scope This International Standard specifies a method for the measurement of trace amounts of basic materials present in polyeth
21、er polyols used in the production of polyurethanes. It is important to know the trace amount of basicity in a polyol to prevent gelation of the reaction mass during the production of polyurethane prepolymers. It is also useful to control the basicity in polyols used for polyurethane production to as
22、sure consistent and reproducible reaction behaviour. This method is suitable for quality control, as a specification test and for research. The applicable range is 0?g to 50?g/g, expressed as KOH. The method is not applicable to amine-based polyols. The values may be reported as CPR (controlled poly
23、merization rate) units. 2Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. How
24、ever, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and
25、 IEC maintain registers of currently valid International Standards. ISO 3696:1987, Water for analytical laboratory use Specification and test methods. ISO 6353-1:1982, Reagents for chemical analysis Part 1: General test methods. ISO 6353-2:1983, Reagents for chemical analysis Part 2: Specifications
26、First series. ISO 6353-3:1987, Reagents for chemical analysis Part 3: Specifications Second series. 3Terms and definitions For the purposes of this International Standard, the following terms and definitions apply. 3.1 polyurethane a polymer prepared by the reaction of an organic di- or polyisocyana
27、te with compounds containing two or more hydroxyl groups Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 08:41:01 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 148
28、99:2001(E) 2 ISO 2001 All rights reserved 3.2 CPR value controlled polymerization rate value the number of microequivalents of base in a 30 g test portion of polyol (i.e. meq of base in 30 kg of polyol) 4Principle A 30 g test portion of polyol is diluted with methanol and titrated with aqueous 0,01
29、mol/l HCl. The results are compared with a blank titration of the methanol. 5Sampling Draw samples from a well-mixed vessel into a thoroughly cleaned and dry borosilicate glass container (soft glass containers are not acceptable). If sampling from a line or valve, flush the line thoroughly with the
30、product before starting to draw the sample. Seal the sample until analysis. 6Interferences Any acidic or basic materials inadvertently introduced into the sample will cause errors in the analysis. Any material capable of serving as a buffer may interfere with the analysis by obscuring the titration
31、end point. Some samples may contain traces of several different compounds which may have the effect of causing multiple breaks in the titration curve, making interpretation difficult. This analysis is not applicable to amine-based polyols. 7Reagents Reagent-grade chemicals shall be used in all deter
32、minations. Unless otherwise indicated, it is intended that all reagents conform to the specifications of ISO 6353-1, ISO 6353-2 and ISO 6353-3, although other grades may be used provided that it is first determined that the reagent is of sufficiently high purity to permit its use without lessening t
33、he accuracy of the determination. Unless otherwise indicated, references to water shall be understood to mean grade 2 reagent water as defined by ISO 3696:1987. 7.1Hydrochloric acid, standard solution, 0,01 mol/l. Prepare and standardize in accordance with good practice, using potassium acid phthala
34、te (7.2) as a primary standard. Standardize to detect changes of 0,000 1 mol/l. 7.2Potassium acid phthalate. Use a certified primary standard. 7.3Methanol, reagent grade, conforming to ISO 6353-2. 8Apparatus 8.1Autotitrator, capable of determining multiple end points, equipped with a pair of electro
35、des or a combination glass calomel electrode, a 5 ml burette and a recorder. 8.2Burette, or other automatic dispensing device, capable of dispensing 50 ml?0,1 ml. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Res
36、ale, 04/23/2007 08:41:01 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 14899:2001(E) ISO 2001 All rights reserved3 8.3Balance, capable of weighing 30 g test portions to?1 mg. 8.4Titration flask, 100 ml, or other suitable titration vessel. 8.5Magnetic stirrer, equipped
37、 with an inert stirrer bar, or equivalent. 9Procedure 9.1Set up the titrator (8.1) for titrations having a maximum titrant volume of 5 ml. 9.2Add 50 ml of methanol (7.3) to a 100 ml titration flask (8.4) for use as a solvent blank. NOTESome popular automatic titrimeters are equipped with 100 ml titr
38、ation vessels. With other titrimeters, an acceptable variation of the method is to use 100 ml of methanol in a 150 ml titration vessel, as is done in JIS K 1557. 9.3Titrate the solvent blank with 0,01 mol/l HCl (7.1) and record the volume of titrant used. The end point is taken as the point of infle
39、ction of the last end point on the titration curve. The blank should consume less than 0,2 ml of 0,01 mol/l HCl. 9.4Into a 100 ml titration flask, weigh about 30 g of sample to the nearest 1 mg. Add 50 ml of methanol and stir until well mixed. (See the note to 9.2.) 9.5Titrate with 0,01 mol/l HCl an
40、d record the volume of titrant up to the last end point. NOTEDepending on the sample being analysed, as many as three inflection points may be seen. Use the last end point. 10 Expression of results 10.1Calculate the CPR value using the following equation: CPR value = SB 30 ()1000VVM m ? where VSis t
41、he volume of HCl needed to titrate the test portion, in ml; VBis the volume of HCl needed to titrate the blank, in ml; Mis the molarity of the HCl, in mol/l; mis the mass of the test portion, in g. 10.2The basicity may also be calculated as?g KOH/g of sample using the following equation: ?g KOH/g of
42、 sample = SB 56,1 ()1000VVM m ? Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 08:41:01 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 14899:2001(E) 4 ISO 2001 All
43、 rights reserved 11 Precision and bias 11.1 Precision 11.1.1Use the criteria for repeatability and reproducibility shown in 11.1.2 and 11.1.3 to judge the acceptability of results. NOTEPrecision data were determined by a round-robin test conducted by eight laboratories using five different commercia
44、lly available polyol samples covering a range of 0,3 CPR units to 1,2 CPR units. Data may be obtained from ASTM Committee D-20 or from the PURMAC committee of the American Plastics Council. 11.1.2Repeatability (single analyst): Duplicate results obtained by the same analyst using the same equipment
45、on the same day should only be considered suspect if they differ by more than 0,2 CPR units. This repeatability was calculated from pooled experimental data following ASTM E 180. 11.1.3Reproducibility (multilaboratory): Results, each the mean of duplicates, obtained on identical test materials in se
46、parate laboratories should only be considered different if they differ from that of another laboratory by more than 0,6 CPR units. This reproducibility was calculated from pooled experimental data following ASTM E 180. 11.2 Bias Bias is the difference between the expectation of the test results and
47、an accepted reference value. The bias of this test has not been determined. 12 Test report The test report shall include the following: a)a reference to this International Standard; b)all details necessary to identify the product analysed; c)the results obtained, expressed as CPR units to the neares
48、t 0,1 CPR unit, or as?g KOH/g; d)any incident or detail not stipulated in this International Standard which may have influenced the result; e)the date of the analysis. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 08:41:01 MDTNo reproduction or networking permitted without license from IHS -,-,